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The  31 P and  13 C NMR spectra of the heteroatom-substituted λ 3 -phosphaalkynes (Me 3 Si)-  i PrNCP (1), K +  [ i PrNCPl -  (2) and KOCP · 2 DME (3) are described (Me = methyl;  i Pr = isopropyl). In addition, 15 N NMR data of 1 and 2 as well as further NMR results of all accessible nuclei of 1 to 3 are reported. The absolute values of the coupling constants  1 J( 31 P 13 C) of 1, 2 and 3, 18.2, 45.7 and 57.2 Hz, respectively, are considerably different; the geminal coupling constants  2 J(  31 P 15 N) of the first two compounds show a decrease in the reverse order, 15.1 and 3.3 Hz.  13 C,  29 Si, 15 N, and  18 O isotope effects on the nuclear shielding of the  31 P nucleus in the non isotope-enriched compounds 1, 2 or 3 are presented and discussed. The [mono-13C]isotopomers of 1, 2 and 3 exhibit extremely negative  31 P 13 C one-bond isotope shifts varying from -211 to -223 ppb. Remarkably, for 1 and 2 large two-bond  31 P 15 N isotope shifts of -32 and -84 ppb, respectively, are observed. An unexpectedly large two-bond  31 P 18 0 isotope effect of -124 ppb was assigned to the [mono- 18 0]isotopomer of compound 3. A three-bond  31 P 13 C isotope shift of -27 ppb was found in 2.

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Remarkably Large  15 N,  13 C and  18 O Isotope NMR Shifts of the Mono-coordinate Phosphorus Atoms in the Compounds (Me 3  Si) i PrNCP, K + [ i PrNCP]-and KOCP · 2 DME (DME = 1,2-Dimethoxyethane)